反应详情

In 1 N aqueous sodium hydroxide (45 ml) is dissolved 1-hydroxy-6-nitro-1,2,3-benzotriazole (7.2 g). To the solution is gradually added p-toluenesulfonyl chloride (7.7 g) with stirring under ice-cooling and further are added thereto ethyl acetate (100 ml) and water (50 ml) and the mixture is stirred for 1 hour. The ethyl acetate layer is separated, dried over magnesium sulfate-charcoal, and concentrated until it becomes about 30 ml. n-Hexane (about 50 ml) is added thereto and the mixture is allowed to stand. The precipitated crystals are separated and dried to give faint yellow needles of 1-(p-toluenesulfonyl-oxy)-6-nitro-1,2,3-benzotriazole (7.5 g), melting point: 142°-144° C. The product is recrystallized from ethyl acetate-n-hexane to give a pure product, melting point: 144° C.

1. temperaturecooling
2. additionfurther are added
3. customThe ethyl acetate layer is separated
4. dry with materialdried over magnesium sulfate-charcoal
5. concentrationconcentrated until it
6. additionn-Hexane (about 50 ml) is added
7. customThe precipitated crystals are separated
8. customdried